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CAS No. : | 93281-65-3 | MDL No. : | MFCD00458267 |
Formula : | C10H14BrNO2S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 292.19 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With tetrakis(triphenylphosphine) palladium(0); copper(l) chloride; lithium chloride at 80℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With scandium tris(trifluoromethanesulfonate) In nitromethane at 50℃; for 4h; | |
91% | With boron trichloride In dichloromethane at 20℃; for 0.5h; | |
91% | With iodine; aluminium In acetonitrile at 80℃; for 18h; chemoselective reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 6 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene 3.1: KHMDS; HMPA / tetrahydrofuran / 0 °C 4.1: LiOH / tetrahydrofuran; methanol / 65 °C 5.1: HCl 6.1: TFA / CH2Cl2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 5 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene 3.1: KHMDS; HMPA / tetrahydrofuran / 0 °C 4.1: LiOH / tetrahydrofuran; methanol / 65 °C 5.1: HCl |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene 3.1: KHMDS; HMPA / tetrahydrofuran / 0 °C 4.1: LiOH / tetrahydrofuran; methanol / 65 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene 3.1: KHMDS; HMPA / tetrahydrofuran / 0 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 7 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene 3.1: KHMDS; HMPA / tetrahydrofuran / 0 °C 4.1: LiOH / tetrahydrofuran; methanol / 65 °C 5.1: HCl 6.1: TFA / CH2Cl2 7.1: EDC; DMAP / CH2Cl2 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 8 steps 1.1: n-BuLi / tetrahydrofuran / -78 °C 1.2: tetrahydrofuran / -78 °C 2.1: SOCl2; (i-Pr)2NEt / toluene 3.1: KHMDS; HMPA / tetrahydrofuran / 0 °C 4.1: LiOH / tetrahydrofuran; methanol / 65 °C 5.1: HCl 6.1: TFA / CH2Cl2 7.1: EDC; DMAP / CH2Cl2 8.1: MMPP / CH2Cl2; methanol |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | In MC at 0 - 20℃; for 1h; Inert atmosphere; | 167.1 Example 167: Synthesis of N -(( E )-5-hydroxyadamantan-2-yl)-6-(( R )-2-methyl-4-(4-sulfamoylphenyl)piperazin-1-yl)picolinamide [378] [379] Step 1: Synthesis of 4-bromo- N -(tert-butyl)benzenesulfonamide [380] 4-bromobenzenesulfonyl chloride (200 mg, 0.783 mmol) was dissolved in MC (10 ml), followed by dropwise addition of tert-butylamine (0.41 ml, 3.91 mmol) at 0oC, and then the resulting mixture was stirred at room temperature under nitrogen stream for 1 hour. Distilled water (15 ml) was added to the resulting reaction liquid, followed by extraction with MC (30 ml x 2). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was dried under vacuum, to obtain 228 mg of white solid (100%). |
100% | In dichloromethane at 0℃; for 0.5h; | 17 Preparation of Compound 17-c At 0° C., 4-bromobenzenesulfonyl chloride (3.0 g, 11.8 mml) was added to a solution of t-butyl amine (2.0 g, 29.6 mmol) in dichloromethane (30 mL) and stirred for 30 minutes. The reaction mixture was washed with aqueous hydrochloride (1 N, 20 mL) and water (30 mL×3) in sequence. The organic layer was dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure to give white solid 17-c (3.6 g, yield: 100%), which was used directly for the next step without further purification. |
98% | In dichloromethane at 0 - 20℃; for 0.5h; | 6.1 Step 1: 4-Bromo-/V-tert-butyl-benzenesulfonamide To a solution of ie/ -butylamine (8.70 g, 12.5 mL, 118.96 mmol) in DCM (100 mL) at 0 °C was added 4-bromobenzenesulfonyl chloride (9.25 g, 36.201 mmol). After 10 min, the cooling bath was removed and the mixture was stirred at room temperature for 20 min. 1 N HC1 (100 mL) was added and the phases were separated. The organic layer was washed with water (100 mL) and dried with MgS04, filtered and concentrated in vacuo to afford 4-bromo- V-ieri-butyl-benzenesulfonamide (10.34 g, 98%) as a white solid. 1H NMR (400 MHz, CDCL) d 7.79 - 7.74 (m, 2H), 7.66 - 7.60 (m, 2H), 4.69 (br. s., 1H), 1.24 (s, 9H). ESI-MS m/z calc. 290.9929, found 236.2 (M- C4H8+H)+; Retention time: 1.79 minutes (LC method E). |
91% | With N-ethyl-N,N-diisopropylamine In dichloromethane at 20℃; for 1h; | |
86% | With triethylamine In dichloromethane at 0 - 20℃; | 20 Place t-butylamine (4.32 mL, 41.1 mmol), triethylamine (8.15 mL, 58.7 mmol) and dichloromethane (75 mL) in a 3-neck round bottom flask. Cool this stirring solution to 0°C and add a solution of 4-bromobenzenesulfonyl chloride (10.0 g, 39. 1 mmol) in dichloromethane (50 mL). Add additional dichloromethane (25 mL) and stir the reaction overnight, allowing it to warm to ambient temperature. Evaporate the reaction in vacuo. Suspend the resulting white solid in ethyl acetate and filter it. Concentrate the filtrate in vacuo and purify the resulting residue by flash chromatography (silica gel ; 50%-80% gradient CH2C12 in hexanes) to provide 9.85 g of 4-bromo-N-tert-butyl- benzenesulfonamide (86%). Place 4-bromo-N-tert-butyl-benzenesulfonamide (2.00 g, 6. 84 mmol), bis (pinacolato) diboron (2.09 g, 8.21 mmol), PdC12 (dppf) 2'CH2CI2 (175 mg, 0.24 mmol), potassium acetate (2.02 g, 20.5 mmol) and anhydrous dimethyl sulfoxide (25 mL) in a round bottom flask. Put the reaction in an oil bath and stir it at 90°C for 7. 5 hours. Cool the purple colored reaction to ambient temperature, quench with ample water and extract the resulting aqueous mixture into dichloromethane. Wash the combined extracts with water and brine; then dry (sodium sulfate) and evaporate them in vacuo. Purify the resulting dark solid on a flash column (silica gel; 0%-5% gradient of EtOAc in CH2C12) to provide 2.00 g of the title compound (86%). |
In tetrahydrofuran; Isopropyl acetate | 33.3 Step 3 Step 3 N-t-Butyl-4-bromobenzenesulfonamide To a solution of 4-bromobenzenesulfonyl chloride (100.2 g) in THF (400 mL) was added t-butylamine (125 mL). An exothermic reaction results with gentle refluxing of the solvent. After 30 min, the bath was removed and the mixture was allowed to warm to r.t. Isopropyl acetate (400 mL) was added and the mixture was washed twice with water. The aqueous phase was back-extracted with ethyl acetate and the combined organics were dried (sodium sulfate) and concentrated to provide the title compound as a solid (112.9 g). | |
In dichloromethane at 20℃; | ||
In tetrahydrofuran for 0.5h; Heating / reflux; | 33.3 Step 3: N-t-Butyl-4-bromobenzenesulfonamide To a solution of 4-bromobenzenesulfonyl chloride (100.2 g) in THF (400 mL) was added t-butylamine (125 mL). An exothermic reaction results with gentle refluxing of the solvent. After 30 min, the bath was removed and the mixture was allowed to warm to r.t. Isopropyl acetate (400 mL) was added and the mixture was washed twice with water. The aqueous phase was back-extracted with ethyl acetate and the combined organics were dried (sodium sulfate) and concentrated to provide the title compound as a solid (112.9 g). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With potassium carbonate In DMF (N,N-dimethyl-formamide) at 20℃; | 9.R' A 15 mL DMF mixture of 4-bromo-N-tert-butyl-benzenesulfonamide (1022 mg, 3.5 mmol), iodomethane (0.44mL, 7 mmol), and K2C03 (987 mg, 7 mmol) is stirred at room temperature overnight. Water and ethyl acetate are added to the mixture. The aqueous layer is extracted several times with ethyl acetate. The combined organic layers are washed with H20 and brine, then dried over Na2S04 and evaporated. The crude product is purified by silica-gel column chromatography (gradient: 100% CH2C12 to 20% EtOAc/ CH2C12) give the intermediate 4-bromo-N-tert-butyl-N-methyl- benzenesulfonamide (1040 mg, 97% yield). MS (ES+) 251.9 (M-tBu)+, NMR (CDC13). |
97% | With potassium carbonate In N,N-dimethyl-formamide at 20℃; | 9 Intermediate Preparation 94-Bromo-N-tert-butyl-N-methyl-benzenesulfonamide Procedure R': A 15 mL DMF mixture of 4-bromo-N-tert-butyl-benzenesulfonamide (1022 mg, 3.5 mmol), iodomethane (0.44 mL, 7 mmol), and K2CO3 (987 mg, 7 mmol) is stirred at room temperature overnight. Water and ethyl acetate are added to the mixture. The aqueous layer is extracted several times with ethyl acetate. The combined organic layers are washed with H2O and brine, then dried over Na2SO4 and evaporated. The crude product is purified by silica-gel column chromatography (gradient: 100% CH2Cl2 to 20% EtOAc/CH2Cl2) give the intermediate 4-bromo-N-tert-butyl-N-methyl-benzenesulfonamide (1040 mg, 97% yield). MS (ES+) 251.9 (M-tBu)+, NMR (CDCl3). |
73% | With potassium carbonate In N,N-dimethyl-formamide at 20℃; for 18h; | 168.1 Example 168: Synthesis of N -(( E )-5-hydroxyadamantan-2-yl)-6-(( R )-2-methyl-4-(4-( N -methylsulfamoyl)phenyl)piperazin-1-yl)picolinamide [387] [388] Step 1: Synthesis of 4-bromo- N -(tert-butyl)- N -methylbenzenesulfonamide [389] 4-Bromo-N-(tert-butyl)benzenesulfonyl amide (100 mg, 0.342 mmol) and potassium carbonate (95 mg, 0.684 mmol) were dissolved in DMF (2 ml), followed by addition of iodomethane (0.043 ml, 0.684 mmol), and then the resulting liquid was stirred at room temperature for 18 hours. Distilled water (10 ml) was added to the resulting reaction liquid, followed by extraction with EtOAc (10 ml x 3). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (20% EtOAc /Hexanes), to obtain 77mg of yellow oil (73%). |
With potassium carbonate In N,N-dimethyl-formamide at 15 - 25℃; for 6h; Inert atmosphere; | 131 Intermediate 131 To a solution of 4-bromo- V-(iert-butyl) benzenesulfonamide (1-35; 1.0 g, 3.4 mmol) and potassium carbonate (0.946 g, 6.84 mmol) in DMF (20 mL) was added methyl iodide (0.428 mL, 6.84 mmol) at room temperature. The reaction mixture was stirred for 6 h, then quenched with water (50 mL) and extracted with ethyl acetate (50 mL x 3), dried over Na2S04, filtered and concentrated in vacuo. The residue was purified by silica chromatography, eluting with 0-10% EtOAc/Hexanes to give 4-bromo-N-(iert-butyl)-N-methylbenzenesulfonamide. 1H NMR (600 MHz, CDC13): δ 7.65 (d, / = 8.8 Hz, 2H), 7.58 (d, / = 8.8 Hz, 2H), 2.94 (s, 3H), 1.32 (s, 9H). | |
With potassium carbonate In N,N-dimethyl-formamide at 15 - 25℃; for 6h; Inert atmosphere; | 4-bromo-N-(tert-butyl)-N-methylbenzenesulfonamide General procedure: To a solution of 4-bromo-N-(ieri-butyl)benzenesulfonamide (1.00 g, 3.42 mmol) and potassium carbonate (0.946 g, 6.84 mmol) in DMF (20 mL) was added methyl iodide (0.43 mL, 6.8 mmol) at room temperature. The reaction was stirred for 6 hours, then quenched by addition of water and extracted with EtOAc (x 3). The organic layers were dried over sodium sulfate, filtered, and concentrated in vacuo and purified by silica chromatrography, eluting with 0-10% EtOAc in hexanes to give 1-12-1. LRMS (ESI) calc'd for CnHi7NBr02SNa [M+Na]+: 328, found 328. 1H NMR (600 MHz, CDC13): δ 7.69 (d, / = 8.7 Hz, 2H), 7.62 (d, / = 8.7 Hz, 2H), 2.97 (s, 3H), 1.35 (s, 9H). | |
With potassium carbonate In N,N-dimethyl-formamide at 20℃; for 6h; Inert atmosphere; | 31-1 4-bromo-N-(ieri-butyl)-N-methylbenzenesulfonamide To a solution of 4-bromo-N-(iert-butyl)benzenesulfonamide (1.00 g, 3.42 mmol) and potassium carbonate (0.946 g, 6.84 mmol) in DMF (20.0 mL) was added methyl iodide (0.43 mL, 6.8 mmol) at room temperature. The reaction was stirred for 6 hours, then quenched by addition of water and extracted with EtOAc (x 3). The organic layers were dried over sodium sulfate, filtered and concentrated in vacuo and purified by silica chromatrography, eluting with 0-10% EtOAc in hexanes to give 1-31-1 as an oil. LRMS (ESI) calc'd for CnHi7NBr02SNa [M+Na]+: 328, found 328. 1H NMR (600 MHz, CDC13): δ 7.69 (d, / = 8.7 Hz, 2H), 7.62 (d, / = 8.7 Hz, 2H), 2.97 (s, 3H), 1.35 (s, 9H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
86% | With potassium acetate In dichloromethane; dimethyl sulfoxide at 90℃; for 7.5h; | 8.P' A 25 mL DMSO mixture of 4-bromo-N-tert-butyl-benzenesulfonamide (CAS 93281-65-3) (2000 mg, 6.84 mmol), bis (pinacolato)diboron mg, 8.21 mmol), [1,1 bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with CH2C12 (1:1) (175 mg, 240 mmol), and KOAc (2020 mg, 20.5 mmol) is stirred under N2 at 90° C for 7.5 hours. Reaction mixture is allowed to cool, is diluted with H20 and is extracted with CH2C12. The CH2C12 extract is washed with H20 and brine, dried (Na2S04) and evaporated. The crude product is purified by silica-gel column chromatography (gradient: 100% CH2C12 to 5% EtOAc/ CH2C12) give the intermediate N-tert-butyl-4-(4,4,5,5- tetramethyl- [1,3,2]dioxaborolan-2-yl)-benzenesulfonamide (2000 mg, 86% yield). (MS (ES-) 256 (boronic acid). |
86% | Stage #1: 4-bromo-N-(tert-butyl)benzenesulfonamide; bis(pinacol)diborane With potassium acetate In dimethyl sulfoxide at 20 - 90℃; for 7.5h; Stage #2: With water In dimethyl sulfoxide | 20 Place t-butylamine (4.32 mL, 41.1 mmol), triethylamine (8.15 mL, 58.7 mmol) and dichloromethane (75 mL) in a 3-neck round bottom flask. Cool this stirring solution to 0°C and add a solution of 4-bromobenzenesulfonyl chloride (10.0 g, 39. 1 mmol) in dichloromethane (50 mL). Add additional dichloromethane (25 mL) and stir the reaction overnight, allowing it to warm to ambient temperature. Evaporate the reaction in vacuo. Suspend the resulting white solid in ethyl acetate and filter it. Concentrate the filtrate in vacuo and purify the resulting residue by flash chromatography (silica gel ; 50%-80% gradient CH2C12 in hexanes) to provide 9.85 g of 4-bromo-N-tert-butyl- benzenesulfonamide (86%). Place 4-bromo-N-tert-butyl-benzenesulfonamide (2.00 g, 6. 84 mmol), bis (pinacolato) diboron (2.09 g, 8.21 mmol), PdC12 (dppf) 2'CH2CI2 (175 mg, 0.24 mmol), potassium acetate (2.02 g, 20.5 mmol) and anhydrous dimethyl sulfoxide (25 mL) in a round bottom flask. Put the reaction in an oil bath and stir it at 90°C for 7. 5 hours. Cool the purple colored reaction to ambient temperature, quench with ample water and extract the resulting aqueous mixture into dichloromethane. Wash the combined extracts with water and brine; then dry (sodium sulfate) and evaporate them in vacuo. Purify the resulting dark solid on a flash column (silica gel; 0%-5% gradient of EtOAc in CH2C12) to provide 2.00 g of the title compound (86%). |
86% | With potassium acetate In dimethyl sulfoxide at 90℃; for 7.5h; Inert atmosphere; | 8 Intermediate Preparation 8N-tert-Butyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzenesulfonamide Procedure P': A 25 mL DMSO mixture of 4-bromo-N-tert-butyl-benzenesulfonamide (CAS 93281-65-3) (2000 mg, 6.84 mmol), bis(pinacolato)diboron (2090 mg, 8.21 mmol), [1,1 bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with CH2Cl2 (1:1) (175 mg, 240 mmol), and KOAc (2020 mg, 20.5 mmol) is stirred under N2 at 90° C. for 7.5 hours. Reaction mixture is allowed to cool, is diluted with H2O and is extracted with CH2Cl2. The CH2Cl2 extract is washed with H2O and brine, dried (Na2SO4) and evaporated. The crude product is purified by silica-gel column chromatography (gradient: 100% CH2Cl2 to 5% EtOAc/CH2Cl2) give the intermediate N-tert-butyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzenesulfonamide (2000 mg, 86% yield). (MS (ES-) 256 (boronic acid). |
68% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate In 1,4-dioxane at 95℃; for 2h; Inert atmosphere; | |
60% | With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate In 1,4-dioxane at 80℃; for 16h; Inert atmosphere; | 17 Preparation of Compound 17-b Under nitrogen, to a suspension of compound 17-c (500 mg, 1.72 mmol), bis(pinacolato)diboron (524 mg, 2.06 mmol) and potassium acetate (505 mg, 5.15 mmol) in 1,4-dioxane (5 mL) was added Pd(dppf)Cl2 (130 mg, 0.17 mmol). The mixture was stirred at 80° C. for 16 hours. After concentration of the mixture under reduced pressure, the residue was diluted with water (50 mL), then extracted with ethyl acetate (50 mL×3). The organic layers were combined and washed with water (50 mL×3) and saturated brine (50 mL) in sequence. After dried over anhydrous sodium sulfate, the mixture was filtrated, the filtrate was concentrated under reduced pressure. The residue was purified by silica column chromatography (petroleum ether:ethyl acetate=5:1) to give white solid 17-b (350 mg, yield: 60%). LC-MS (ESI): m/z=340 [M+H]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; methylmagnesium bromide In tetrahydrofuran; Isopropyl acetate; water; toluene | 33.4 Step 4 Step 4 4-t-Butylaminosulfonylbenzene boronic acid To a solution of N-t-butyl-4-bromobenzenesulfonamide from Step 3 (60.2 g) in THF (700 mL) at 0° C. was added methyl magnesium bromide (75 mL of a 3 M solution in THF). The mixture was stirred at r.t. for 15 min and then cooled to -65° C. n-Butyl lithium (2.35 eq as a solution in hexanes) was added dropwise over 45 min and after addition was complete, the mixture was stirred at -72° C. for 30 min. Triisopropoxyborate (190 mL) was added slowly while the reaction mixture temperature rose to -58° C. Upon completion of the addition, the cold bath was removed and the mixture was warmed to r.t. Concentrated NH4 Cl (500 mL), water (500 mL) and 2N HCl (500 mL) were added successively and then the mixture was adjusted to pH 5-7 with 10 N NaOH. The resulting mixture was stirred at r.t. for 15 h and then isopropyl acetate (700 mL) was added. The aqueous layer was acidified to pH 3 and the phases were separated. The aqueous layer was further extracted with isopropyl acetate/t-butanol (1:1, 600 mL). The combined organics were dried (sodium sulfate) and concentrated. The residue was stirred vigorously in toluene (300 mL) and filtration of the resulting solid provided the title compound (42 g). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | With lithium bromide; zinc dibromide In tetrahydrofuran; 1-methyl-pyrrolidin-2-one at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | With lithium bromide; zinc dibromide In tetrahydrofuran; 1-methyl-pyrrolidin-2-one at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: potassium carbonate / N,N-dimethyl-formamide / 18 h / 20 °C 2: caesium carbonate / 2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl; dichlorobis(tri-O-tolylphosphine)palladium / toluene / 18 h / 90 °C / Inert atmosphere 3: trifluoroacetic acid / 2 h / 90 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: potassium carbonate / N,N-dimethyl-formamide / 18 h / 20 °C 2: caesium carbonate / 2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl; dichlorobis(tri-O-tolylphosphine)palladium / toluene / 18 h / 90 °C / Inert atmosphere |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: caesium carbonate / 2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl; dichlorobis(tri-O-tolylphosphine)palladium / toluene / 15 h / 90 °C / Inert atmosphere 2: trifluoroacetic acid / MC / 15 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With caesium carbonate In toluene at 90℃; for 15h; Inert atmosphere; | 167.2 Step 2: Synthesis of 6-(( R )-4-(4-( N -(tert-butyl)sulfamoyl)phenyl)-2-methylpiperazin-1-yl)- N -(( E )-5-hydroxyadamantan-2-yl)picolinamide [382] N-((E)-5-hydroxyadamantan-2-yl)-6-((R)-2-methylpiperazin-1-yl)picolinamide(30 mg, 0.0810 mmol), 4-bromo-N-(tert-butyl)benzenesulfonyl amide (28 mg, 0.0972 mmol), Pd[P(o-tolyl)3]2Cl2 (1 mg, 0.000810 mmol), BINAP (3 mg, 0.00486 mmol), and cesium carbonate (26 mg, 0.0810 mmol) were suspended in toluene (5 ml), and then the resulting liquid was stirred at 90oC under nitrogen stream for 15 hours. The resulting reaction liquid was concentrated under reduced pressure, and then the residue thus obtained was subjected to MPLC (5% MeOH/MC), to obtain 45 mg of pale yellow solid (96%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate / 1,4-dioxane / 16 h / 80 °C / Inert atmosphere 2: sodium carbonate; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / water; ethanol / 16 h / 80 °C / Inert atmosphere 3: toluene-4-sulfonic acid / butan-1-ol / 16 h / 110 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate / 1,4-dioxane / 16 h / 80 °C / Inert atmosphere 2: sodium carbonate; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / water; ethanol / 16 h / 80 °C / Inert atmosphere |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With dichlorobis(tri-O-tolylphosphine)palladium; caesium carbonate; 2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl In toluene at 90℃; for 15h; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89% | Stage #1: (S)-2-trifluoromethyl-oxirane With n-butyllithium In tetrahydrofuran; hexane at -50℃; for 0.00555556h; Schlenk technique; Inert atmosphere; Flow reactor; Stage #2: With zinc(II) chloride In tetrahydrofuran; 2-methyltetrahydrofuran; hexane at -50℃; for 0.0277778h; Inert atmosphere; Schlenk technique; Flow reactor; Stage #3: 4-bromo-(N-tert-butyl)benzenesulfonamide With C47H59N3O3PPdS In tetrahydrofuran; 2-methyltetrahydrofuran; hexane; toluene at 40℃; Inert atmosphere; Sealed tube; Flow reactor; enantioselective reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: potassium acetate; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / 1,4-dioxane / 2 h / 95 °C / Inert atmosphere 2: sodium carbonate; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / water; 1,4-dioxane / 2 h / 95 °C / Inert atmosphere 3: boron trichloride / dichloromethane / 0.5 h / 0 °C / Inert atmosphere |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: potassium acetate; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / 1,4-dioxane / 2 h / 95 °C / Inert atmosphere 2: sodium carbonate; (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride / water; 1,4-dioxane / 2 h / 95 °C / Inert atmosphere |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
59% | Stage #1: 4-bromo-(N-tert-butyl)benzenesulfonamide With n-butyllithium In tetrahydrofuran; hexane at -100℃; Stage #2: chloro-trimethyl-silane In tetrahydrofuran; hexane at -100 - 20℃; for 0.5h; | 6.2 Step 2: /V-tert-Butyl-4-trimethylsilyl-benzenesulfonamide To a solution of 4-bromo- V-/eri-butyl-benzenesulfonamide (5 g, 17.112 mmol) in tetrahydrofuran (50 mL) at -100 °C (liquid N2 + ether) was added n- butyllithium (1.6 M in hexane) (25 mL, 40.00 mmol) dropwise and the reaction was stirred at this temperature for 30 minutes. Trimethylsilyl chloride (4.280 g, 5 mL, 39.39 mmol) was then added, the reaction was allowed to warm to room temperature and stirred for 30 minutes. The solution was quenched using an aqueous HC1 6N solution (20 mL) and extracted with EtOAc (100 mL). The organic phase was washed with a saturated aqueous NH4Cl solution (5 x 50 mL) and brine (100 mL), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica-gel column chromatography on a SNAP 100 g and GOLD 120 g column, eluting from 0% to 15% of ethyl acetate in heptanes to afford N-tert-butyl-4- trimethylsilyl-benzenesulfonamide (2.9 g, 59%) as a white solid. 'H NMR (400 MHz, CDCL) d 7.85 (d, J = 8.3 Hz, 2H), 7.63 (d, J = 8.3 Hz, 2H), 4.53 (s, 1H), 1.25 (s, 9H), 0.30 (s, 9H). ESI-MS m/z calc. 285.1219, found 230.2 (M-55)+; Retention time: 1.95 minutes (LC method E). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
52% | Stage #1: 4-bromo-(N-tert-butyl)benzenesulfonamide With n-butyllithium In tetrahydrofuran; hexane at -95℃; for 0.666667h; Stage #2: trimethylbromogermane In tetrahydrofuran; hexane at -95℃; for 0.333333h; | 14.1 Step 1: /V-tert-Butyl-4-trimethylgermyl-benzenesulfonamide A solution of 4-bromo-/V-/eri-butyl-benzenesulfonamide (3.4 g, 11.64 mmol) in THF (70 mL) was cooled to -95 °C, and then a solution of H-butyllithium in hexane (11 mL of 2.5 M, 27.50 mmol) was added drop-wise over ten minutes. The pale yellow solution was stirred for thirty minutes at -95 °C, then bromo(trimethyl)germane (5 g, 25.297 mmol) was added drop-wise over five minutes and the resulting mixture was stirred for 15 minutes at -95 °C. The reaction mixture was warmed to 10 °C and quenched with 70 mL of 1M hydrochloric acid, then was extracted with dichloromethane (3 x 25 mL). The aqueous phase was discarded and the combined organic phases were dried over sodium sulfate and concentrated in vacuo to obtain a yellow oil that was purified by silica gel chromatography to obtain A/-//7-butyl-4-tri mcthylgcrmyl- benzenesulfonamide (2.1 g, 52%). ESI-MS m/z calc. 331.0661, found 332.9 (M+2)+; Retention time: 6.26 minutes (LC method C). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / -100 °C 1.2: 0.5 h / -100 - 20 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 2 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / -100 °C 1.2: 0.5 h / -100 - 20 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 2 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / 0.67 h / -95 °C 1.2: 0.33 h / -95 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 22 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / 0.67 h / -95 °C 1.2: 0.33 h / -95 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 22 h / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / -100 °C 1.2: 0.5 h / -100 - 20 °C 2.1: trifluoroacetic acid / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / -100 °C 1.2: 0.5 h / -100 - 20 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 2 h / 20 °C 4.1: potassium carbonate / dimethyl sulfoxide / 16 h / 150 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / -100 °C 1.2: 0.5 h / -100 - 20 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 2 h / 20 °C 4.1: potassium carbonate / dimethyl sulfoxide / 16 h / 150 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / 0.67 h / -95 °C 1.2: 0.33 h / -95 °C 2.1: trifluoroacetic acid / 20 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: n-butyllithium / tetrahydrofuran; hexane / 0.67 h / -95 °C 1.2: 0.33 h / -95 °C 2.1: trifluoroacetic acid / 20 °C 3.1: 1,1'-carbonyldiimidazole / tetrahydrofuran / 1 h / 20 °C 3.2: 22 h / 20 °C 4.1: potassium carbonate / dimethyl sulfoxide / 16 h / 150 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene In 1,4-dioxane at 100℃; | 12 Preparation of tert-butyl 1-(4-(N-tert-butylsulfamoyl)phenyl)-2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate A mixture of 262 mg tert-butyl 2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate (1.0 mmol, 1.0 equiv), 290 mg 4-bromo-N-tert-butylbenzenesulfonamide (10.0 mmol, 1.00 equiv), 91.5 mg tris(dibenzylideneacetone)dipalladium (0.1 mmol, 0.1 equiv), 115 mg 4,5- bis(diphenylphosphino)-9,9-dimethylxanthene (0.2 mmol, 0.2 equiv) and 276 mg cesium carbonate (2.0 mmol, 2.00 equiv) in 20 mL dioxane was stirred at 100 °C overnight. The mixture was diluted with 100 mL ethyl acetate and washed with 3 x 100 mL volumes of water. The organic phase was concentrated and the residue was purified by column chromatography on silica gel (petroleum ether:ethyl acetate (3:1, v:v)) to yield 283 mg tert-butyl 1-(4-(N-tert- butylsulfamoyl)phenyl)-2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate as a white solid (60 % yield). MS (ESI+) m/z 474 [M+H]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene In 1,4-dioxane at 100℃; | 13 Preparation of tert-butyl 2-(4-(N-tert-butylsulfamoyl)phenyl)-3-oxo-2,3,4,5- tetrahydro-1H-benzo[c]azepin-4-ylcarbamate A mixture of 276 mg tert-butyl 2-oxo-1,2,3,4-tetrahydroquinolin-3-ylcarbamate (1.0 mmol, 1.0 equiv), 290 mg 4-bromo-N-tert-butylbenzenesulfonamide (10.0 mmol, 1.00 equiv), 91.5 mg tris(dibenzylideneacetone)dipalladium (0.1 mmol, 0.1 equiv), 115 mg 4,5- bis(diphenylphosphino)-9,9-dimethylxanthene (0.2 mmol, 0.2 equiv) and 276 mg cesium carbonate (2.0 mmol, 2.00 equiv) in 20 mL dioxane was stirred at 100 °C overnight. The mixture was diluted with 100 mL ethyl acetate and washed with 3 x 100 mL volumes of water. The organic phase was concentrated and the residue was purified by column chromatography on silica gel (petroleum ether:ethyl acetate (3:1, v:v)) to yield 292 mg tert-butyl 2-(4-(N-tert- butylsulfamoyl)phenyl)-3-oxo-2,3,4,5-tetrahydro-1H-benzo[c]azepin-4-ylcarbamate as a white solid (60 % yield). MS (ESI+) m/z 488 [M+H]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
49% | With lithium tetrafluoroborate; 12-phenyl-12H-benzo[b]phenothiazine In dichloromethane at 20℃; for 24h; Irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
89.8% | With tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene In 1,4-dioxane at 100℃; for 2h; Inert atmosphere; | 4.1.1. Procedure for the synthesis of intermediates 2a-r General procedure: To a stirred solution of 3- bromo-N- (tert butyl) benzenesulfonamide (1.1 g, 3.8 mmol) and 4-amino-2-chloro-5-methylpyrimidine (0.6 g, 4.2 mmol) in 1,4- dioxane (20 mL) was added cesium carbonate (2.5 g, 7.6 mmol), tri(dibenzylacetone)diphenyl palladium (0.1 g, 0.1 mmol) and 4,5- diphenylphosphine-9,9-dimethoxyanthracene (0.2 g, 0.3 mmol). The mixture was stirred at 100 °C for 2 h under N 2 atmosphere. Then, the mixture was cooled to room temperature, filtered (the filter cake was washed with dioxane, 10 mL ×3) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2.1: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 1 h / 20 °C 3.2: 24 h 4.1: potassium hydroxide; hydroxylamine hydrochloride / methanol / 2 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2.1: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 1 h / 20 °C 3.2: 24 h 4.1: potassium hydroxide; hydroxylamine hydrochloride / methanol / 2 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3: potassium hydroxide; hydroxylamine hydrochloride / methanol / 2 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2.1: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 1 h / 20 °C 3.2: 24 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2.1: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 1 h / 20 °C 3.2: 24 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 3 steps 1.1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2.1: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 1 h / 20 °C 3.2: 24 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 4 steps 1.1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2.1: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C 3.1: 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 1 h / 20 °C 3.2: 24 h 4.1: potassium hydroxide; hydroxylamine hydrochloride / methanol / 2 h |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: caesium carbonate; tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene / 1,4-dioxane / 2 h / 100 °C / Inert atmosphere 2: trifluoroacetic acid / isopropyl alcohol / 2 h / 80 °C |
Tags: 93281-65-3 synthesis path| 93281-65-3 SDS| 93281-65-3 COA| 93281-65-3 purity| 93281-65-3 application| 93281-65-3 NMR| 93281-65-3 COA| 93281-65-3 structure
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